Jian-Quan Liu,Xinyi Chen,Andrey Shatskiy,Markus D. Kärkäs,Xiang-Shan Wang
A silver-mediated reaction between 2-ethynyl-3-(1-hydroxyprop-2-yn-1-yl)phenols or 2-ethynyl-3-(1-hydroxyprop-2-yn-1-yl)anilines and methylene isocyanides has been developed. A sequential 5-endo-dig cyclization and [3 + 2] cycloaddition process is proposed. This synthetic strategy is atom- and step-efficient and applicable to a broad scope of substrates, allowing the synthesis of valuable substituted benzofuran- and indole-pyrroles in moderate to high yields.
Xiaolan Feng,Lijun Wang,Xiandong Yao,Huaping Dong,Xiaoxia Wang,Yusen Wang
In this work, we demonstrate that solid-base such as amino-modified silica aerogel (SA-NH 2 ) together with trace water showed excellent catalytic performance in one-pot sequential reaction of acid-catalyzed benzaldehyde dimethyl acetal hydrolysis and base-catalyzed Henry reaction which was usually catalyzed by acid-base bifunctional heterogeneous catalyst. The role of trace water in the reaction was discussed by batch control experiment. This SA-NH 2 /water catalytic system showed high reactant conversions (> 99%) and main product selectivities (up to 99.4%). The trace water induced acid catalysis mechanism and a possible H + /-NH 2 coexistence mechanism were given to explain the synergistic catalytic effect of solid-base and trace water.
In this study, a hydroxypropyl-β-cyclodextrin (HP-β-CD) functionalized monolithic capillary column was prepared by one-pot sequential reaction for the first time. The preparation of the HP-β-CD functionalized monolithic column involves two sequential reactions in one pot: (1) the ring opening reaction between HP-β-CD and glycidyl methacrylate (GMA) catalyzed by 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU); (2) the copolymerization of GMA-HP-β-CD, ethylene dimethacrylate (EDMA) and 2-acrylamido-2-methyl propane sulfonic acid (AMPS). A series of monolithic columns were successfully prepared by varying the temperature of the ring opening reaction or several copolymerization parameters (the type and composition of porogenic solvents, ratio of GMA-HP-β-CD to EDMA and polymerization temperature). Then, the morphologies and structures of the resulting monolithic stationary phases were characterized by optical microscopy, scanning electron microscopy (SEM) and nitrogen adsorption analysis. Raman spectroscopy clearly indicated the successful bonding of HP-β-CD onto the monolith. When the prepared chiral stationary phase (CSP) was applied for the separation of a set of racemic compounds by capillary electrochromatography (CEC), including racemic anticholinergic drugs, β-adrenergic drugs, meptazinol and its intermediates, satisfactory separation selectivities were obtained. Additionally, the column also showed excellent separation abilities towards four flavanone glycosides epimers. Furthermore, the prepared monolithic columns exhibited satisfactory stability and reproducibilities of retention time, resolution and column efficiency. These results demonstrated the potential and usefulness of the developed one-pot sequential strategy in the preparation of other derivatized CD functionalized monolithic columns.
PVAc-based inverted core/shell (ICS) structured latex adhesive with improved water- and heat-resistance was prepared by a copolymerizing-grafting sequential reaction approach. The sequential reaction process combines the function of a copolymer layer and an active grafting site to controllably achieve the thermodynamic non-equilibrium ICS morphology with hydrophilic poly(vinyl acetate) (PVAc) cores and hydrophobic polystyrene (PS) shells. The difference between the sequential reaction approach and the chemical grafting method was explored. Structured latex particle morphology , transferring from strawberry-like particles, over particles with large and irregular PS protuberances, to nearly spherical particles with a smooth surface, was microscopically visualized by changing the amount of butyl acrylate (BA) in the PVAc copolymer cores. The heat- and water-resistant bonding of PVAc-based adhesives on wood blocks were evaluated by shear strength at both dry and wet conditions, as well as the boiling water failure time. The results showed that a significant improvement of water- and heat-resistance, especially for boiling water resistance, was successfully obtained. This novel approach paves a way for controlled design and manufacture of high-performance emulsion adhesives through tailoring particle morphology.
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